Hydrogenation of fatty substances.



J B0YCEL HYDROGENATION 0F FATTY SUBSTANCES. APPLICATION FILED MAR. H1912.

UWTNESSES:

awwi Patented Jan, 14,1919.

2 SHEETS-SHEET I.

J. BOYCE.

HYDROGENATION 0F FATTY SUBSTANCES.

APPLICATION man 11111.1, 1912.

mmmfimmq 1111 11111 1111. 11,1919.

\ 2 SHEETS-SHEET 2.

ll ll n, I All H WITNESSES: INVENTORZ 1W 7 2 g 1' 1 v f 7% M/W ans BUYCJE, or cnrcaeo, rumors. ASSIGNOR TO mamas current on. conra,

@F GUTTJENBERG, NEW JERSEY. A CORPORATION OF NJEW JERSEY.

HYDROGENATION 01E FATTY SUBSTANCES.

Specification of Letters Patent.

lPa-tented Gian. it, into.

Application filed March 7, 1912. Serial No. 682.162.

To all whom it may concern:

Be it known that l, dlAMlcs Boron, a citizen of the United States. and resident of Chicago, county of (Took. State of lllinois, have invented certain new and useful linproveme'nts in the Hydrogenation of Fatty Substances; and l do hereby declare the following to be a full. clear, and exact description of the invention. such as will enable others skilled in the art to which it appertains to make and use the same.

My present'invention relates to a method of hydrogenizing unsaturated fatty acids or their glycerids'by means of hydrogen in the presence of finely divided catalytic material, my object being to produce a high grade product; to operate efficiently. economically and rapidly; to maintain the cataglyzer in edective condition during a long period of use; to safeguard the operation against the danger of explosion: and to utilize the hydrogen continuously as it is produced in spite of local interruptions of the process, such as are. required for changing and removing the material to be treated. thereby avoiding the need of storing amounts of hydrogen in tanks or gas-clusters.

My invention involves the introduction of a stream of hydrogen into the material to he treated containing the finely divided catalyzer. The material may be herein referred to as oil, since an oil. such as cottonseed oil.

is representative of such materials.

First: it provide means for thoroughly subdividing or atomizlng the hydrogen before it passes up into the main body of the oil.

which is in the form of a deep pool or column, and for distributing the hydrogen. so atomized, over the entire cross-sectional area of the'colnrnn at the bottom thereof, whereby the hydrogen may permeate all parts of y the column, rising up through it in a finely divided and thoroughly distributed condi-v tion. I I

Second: To facilitate and render more eflective the aforesaid permeation of the oil by the hydrogen, and also to secure. other re- Third: ll also provide a series of tanks operating in succession, .with means for applying the vacuum suction to anyone of the series While it is in communication with a previous tank. \vhercb any surplus or overflow of hydrogen from one tank may be drawn into and used in a succeeding tank.

By this means, the hydrogen -may be constantly produced and constantly used as it is produced, without resort to the storage of a quantity of hydrogen in a tank or gasholder. I

Fourth: ll also both draw off from and introduce the charge of oil to a tank, while it is still under vacuum. whereby the hot fat is prevented from becoming rancid by oxidation, and the catalyzer from being poisoned which would tend to reduce its elliciency and shorten its life.

Fiftl'i: The catalyzer. which is mingled with the oil in a finely divided condition, it permit. to settle out therefrom by gravity. by

permitting the oil to stand for the required to the sides of the tank or may settle upon the cooling coil. might be drawn ofi' with the oil, but it can readily be separated thtu'efrom by well known clarifying means. 7

ll prefer to use nickel for the eatalyzer. the same being deposited on pumice stone. in any of the Well-known ways. the pumice stone hein first crushed into fine particleseach of w ich will form a small core of hard stone coated with a surface of nickel. This will expose a large surface area of catalytic. metal to the oil, and the catalyzer will settle out from theoil clearly and in a short time.

Tn the accompanying drawings- Figure i represents a front elevation.

partly in section. of suitable apparatus for the practice of the invention:

Fig. 2 represents a top plan \ieuthercof; and i Fig. 3 represents, on a somewhat larger scale, a cross-sectional view. partlybroken away, on the line 3-3 of Fig. 1.

Similar letters of reference indicate similar parts throughout the several views.

an area substantially equal to the cross section of the column. This screen is shown at e in the accompany drawing as supported by a spider .2 (Fig. 3) which, in turn, rests upon a suitable angle iron or other support on the interior wall of tank A.' The hydrogen is admitted below this screen into a space d by a pipe 0, and hydrogen-distributing fan-blades l aremounted below the screen on a vertical'shaft m, which passes through a suitable stufiing box n and which is adapted to be rotated by a driving pulley p or other suitable source of power.

The hydrogen emerges from the pipe 0 in large bubbles which are immediately caught by the slowly revolving fan-blades and thereby swept across the under side of the screen and broken up by the screen into a multitude of fine bubbles which pass upward therethrough. Thus the hydrogen becomes distributed over the cross-sectional area of the column and at the same time is finely subdivided or atomized. It then rises up from the screen through all parts of the column uniformly'and in a. thoroughly subdivided condition. -While this resultant effeet is comparable broadly to that of an ordinary manifold of perforated pipe, such as is-"frequently used for distributing: and subdividing gases employedfor the treatment of liquid, yet my device has this improved characteristic that the gas instead of issuing fromthe perforations of a. maniabout 5 fold, which'are spaced at definite intervals apart, rises from the upper surface of the screen as a mass of fine bubbles more thor oughly and more uniformly distributed over the cross-section of the column into which The second feature of my invention is carried out 'by mainta' .a partial vacuum in the tank'A above theoil column,

that portion of the' tank being connected with the vacuum main C -by means ofa branch pipe f containing a cock 9. So long 7 as the hydrogenizing operation is in progress, this-vacuum is maintainedby the suctlon of branch pipe f-, or, after hydrogen is in excess, by suction through'a succeeding tank. I preferably employ' a' vacuum of or 6 inches (If-mercury and introduce the hydrogen under a. slight pressure,'-

\ about 10 inches of water. This will about.

neutralize the weight of 'an oil column of 84 Inches, while the gas bubbles, being relieved of the air pressure in thespace above the oil column, will expand freel as they enter and pass'thro h the oil. also motesthe comp ete exposure of the oil to thehydrogeml r menses III. For the third feature of my invention, I provide a series of tanks A, six being shown in the drawing, each one of which has an individual branch pipe f with a cock 9 therein connecting it with the exhaust main C. The tanks are also connected together sweat-23m, in a circuit by pipes 71., each containing a cock 2', one end of each pipe h communicating with the interior space, above the oil, of one tank and its other end communicating with the'gas-inflow pipe 0 of the next succeeding tank in the series. Each pipe 72. has also a connection with the gas supply main B 'by means of a pipe a containing a cock 5, whereby the hydrogen supply for each tank may be drawn either directl from main B through pipes a and h, or rom the next precedin tank in the series through pipe h. Oil is introduced into each tank A through an inlet .3 and withdrawn through an outlet t at the bottom just above screen 0.

In the arrangement, any tank of the series may be considered as the starting point of the operation, being first charged about to the level indicated in the first tank at the left of Fig. 1, by pumping in oiL through inlet 8. The oil will also contain the finely subdivided catalyzer, which is preferabl introduced therein after first having een mixed with a small quantity of oil. The gas, admitted by the pipe 0 to the tank so charged, will be distributed and atomized, in the manner above described, by the fanblades Z and the screen 2, and, passing up through the oil will be at first completely tank will be drawn into the second tank an there utilized as in the first one.

The vacuum will be maintained in both tanks at the same point-say 5 to 6 inches of mercury, the suction at the second one being at 10 to 12 inches of mercury to produce the five-inch to six-inch vacuum in .both tanks, and-so on through the series.

In-the same way, three or more tanks can be in operation simultaneously but at different stages of progress of the operation and when the h drogcnizing in the first tank is complete it can be cut out from the series for the p so of drawing ofi therefrom the treated oil and for the introduction of a fresh charge, thou h it is still maintained under vacuum, as .be hereinall till

Lanna i after described. ll) thismeans, l[ am enabled tocontiuuously make use of the hydrogen as it is produced, that portion which is in excess at one tank being taken over into the succeeding tank or tanks. This avoids thenecessity of storing the hydrogen in quantity either before or after it passes through a tanln This is of special importance when the process is carried on in a city or town Where the storing-of hy drogen is prohibited by law. Practically, my process goes on continumisly. each tank being recharged.'after the oil therein-has been treated and drawn off, and itwill then become a succeeding tank with respect to those wherein the hydrogcnizing is still in progress. llor convenience of explanation. however, I have considered the first starting up of the operation. beginning at some one tank which l have referred to as the first one. v

TV. The fmlrthfeature of ,my invention involves. the drawing off of. the oil. after the hydrogenizing is finished. while the 1 tank is still under vacuum, and the subsequent recharging while the vacuum is still maintained. A pump (not shown) will-be connected to the oil outlet t, and the oil pumped out, while the vacuum suction is continued through pipe 7. the tank being out off from the others of, the series by closing cocks i and '1), while cock 9' in the vacuum pipe 0 is opened. The outlet 1% is located near the bottom of the tank .iust.

above the screen 1?, so that practically all of the oil will be drawn off, leaving only a small amount in the space (Z under-the screen with the catalyzer. which has. been allowed to settle out of the oil after the hydrogenizing is finished and before the oil is drawn ofi'. After the oil is withdrawn, (the catalyzer still remaining in the tank to be used again and repeatedly as many times as it will serve before being rc placed,) the outlet t is closed, and, while the vacuum is still maintained, the fresh charge of oil is introduced through the inlet .9 and the described operation repeated.

By this means ll preserve the quality of the product, since it is not subjected to the oxidizing effect of the air which would tend to make it rancid, particularly the thin films of oil clinging-to the walls of the tank and on the cooling coil. lit also preserves the quality of the catalyzer which thus cannot become poisoned by contact withthe air.

till

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V. The sixth feature of my invention resides in the maintaining of the catalyzer continuously in the tank or vessel wherein the hydrogenizing takes place, by allowin it to settle down 1n the bottom of that tan or vessel by gravity before the saturated oil is drawn oh. This is in contrast to the drawing ofi of the catalyzer with the oil and the subsequent separating of it from the oil a filter-press or other process. in furtherance of this end, l find it. of advantage to deposit the catalytic metal, preferably nickel, on pumice stone. Since the depositing of a nickel catalyzer on pumice stone is not new, I do not prescribe any particular method therefor. A catalyzcr thus deposited on pumice stone will settle out completely and in a short time from a body of oil and collect at the bottom of the tank; I may add that the coating of a hard body such-as pumice stone with the catalytic metal exposes an increased surface of contact to thehydrogcn and oil, the action hill till

rises from said space into the main body-portion of the column above; substantially as described.

The method of hydrogenizing fatty substances, which consists in passing upwardly into at liquid column thereof, in which a catalyzingagent is contained, a substantially equally distributed multitude of connninuted hydrogen gas bubbles; substantially as described.

3. The method of hydrogenizing fatty substances which consists in introducing the hydrogen to the bottom of a liquid column of the material to be treated containing a catalyzing agenu'and mechanically distributing and subdividing the gas over the cross-sec tional area of the column, whereby the gas will rise up through all parts of the column in .a finely subdivided condition; substantially sis-described.

4.. in a hydrogenation of a liquid column of fatty substances, the method of distributing: the gas over the cross-sectional area of the column before passingit upwardly therethrough, which consists in dividing off the lower portion of the column from the main body by a screen, admitting the hydrogen below the screen and carrying the hydrogen around in said lower portion thereby subdividin it therein into a multitude of small bubbles; substantially as described.

5. The method of hydrogenizing fatty substances which consists in passing hydrogen gas into a liquid colu thereof in which a catalyzing agent is contained while maintaining the treated liquid under exhaust;

substantially as described.

lltl

lltltl 6. The method of hydrogenizing fatty substances, which consists in passing upwardly into a liquid column thereof, in which a catalyzing, agent is contained, a substan tially equally distributed multitude of hydrogen as bubbles, and maintaining the treated liquid under exhaust, so as to cause a greater expansion of the bubbles on their passage upward; substantially as described.

7. The method of hydrogenizing fatty substances, which consists in passing hydrogen gas' intoa liquid charge thereof, in which a catalyzing agent is contained, while maintaining the liquid charge treated under exhaust, and, after the liquid charge begins to give 01? unabsorbed or surplus hydrogen, passing said surplus into a second liquid charge under exhaust; substantially as described. I

8. The method of hydrogenizing fatty substances, which consists in arranging in sequence a plurality of individual .liqui: charges thereof, each liquid charge containing a catalyzing agent, passing freshly generated hydrogen gas into one of said liquid charges, and passing the unabsorbed or surplus gas therefrom into a succeeding liquid charge ,of the series, until the desired hydrogenation of the initial liquid charge has been effected, such surplus gas being absorbed in the series; substantially as described.

9. The method of hydrogenizing fatty substances, which consists in continuously producing a supply of hydrogen and continuously consuming the same in a series of individual charges of the substances to be treated, by periodically connecting to the series a fresh charge containing a catalyzing agent to receive the surplus hydrogen from a previously comiected charge, and periodically removing from the series a charge wherein the desired hydrogenation has been completed, whereby the storage of hydrogen may be avoided; substantially as described.

10. The method of hydrogenizing successive liquid charges of fatty substances in the same receptacle, which consists in passing hydrogm gas through an initial charge in which a catalyzing agent is contained, re-

menace moving the charge so treated, and admitting the next succeeding charge, while excluding air from the treating receptacle; substantially as described.

11. The method of hydrogenizing successive liquid charges of fatty substances in the same receptacle, which consists in passing hydrogen as through an initial charge containing a ivided catalyzer, separating the catalyzer from the substance within said receptacle, removing, the substance from the receptacle, leaving the catalyzer therein, and recharging the receptacle, air being excluded from the receptacle during each of the aforesaid steps; substantially as described.

12. The method of treating successive charges offatty substances in the same receptacle, which consists in passing hydrogen gas through an initial charge in the presence of a catalyzing agent, permitting the catalyzing agent to settle out of the charge after the desired hydrogenation thereof has been effected, drawing off the substantially clear portion of the charge, and then admittingi into the receptacle a succeeding charge for like hydrogenation; substantially as described.

13. The method of hydrogenizing a fatty substance, which consists in minglin with it a finelydivided catalyzer and sub]ectin the mixture to the action of hydrogen unti In testimony whereof I afiix my signature,

in presence of two witnesses.

' JAMES BOYCE. Witnesses:

JOHN C. PENNIE, MINERVA LOBEL. 

